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. Patented May 20,1919.

liv cnlor F. W. SPERR, In.

DISTILLATION TUBE.

wrucumwmso JAN. 25. m1.

v WzinessS aw Amw- UNITED STATES PATENT OFFICE.

FREDERICK W. SPERB. JR. OF

OAKMONT. PENNSYLVANIA. ASSIG-NOB TO H. KOPPERS COMPANY. OF PITTSBURGH. PENNSYLVANIA. A CORPORATION OF PENNSYLVANIA.

DISTILLATION-TUBE.

Specification of Letters Patent.

' Application filed January 25. 1917. Serial no. 144.431.;

panying drawings, forming part of this specification, in which- Figure 1 is an elevation of the outer tube; Fig. 2 is an elevation of the inner tube; Fig.3 is a sectional view showing the assembled tube complete;

Fig. 4 is an end view of the outer tube; and

Fig. 5 is aiiencl view of the inner tube. The present invention relates to distillation tubes and more particularly to tubes for experimental coal distillation.

In the laboratory testing of coal. it has been the practice to distil a sample in a tube to determine the yield of the various byproducts, such as gas, tar, ammonia, benzol, etc. Glass anclfmetal distillation tubes have been used. Metal tubes have the disadvantage that the sample of coal is distilled under different. conditions from those which obtain in actual practice. Uusually on a large scale! coal is distilled. in fire clay retorts, in chambers, or ovens linedwith fire brick or silica brick. Thus, almost always the vdistillation is carried on in the presence of some material of a silicious nature. Experience has shown that the gases and byproducts are differently affected than is the case when they are in contact with other kinds of material, such as metallic surfaces. Since it is the purpose of making the labora-. tory tests to obtain on a small scale results which will represent or be comparative with those obtained on a large scale with the same kind of coal, it is essential that the laboratory apparatus be constructed ofa material similar to the apparatus used on the large scale commercial practice. Thus. tubes made of glass, fire clay, quartz, etc. are satisfactory for experimental coal distillation. Glass tubes are the most readily obtainable. but it is diflicult to obtain glass tubes of sufiicient refractoriness to withstand the high temperatures at which the coal should be distilled. Very refractory glass tubes are costly. and become distorted in heating. In the method of testing, some of the tarry Patented May 20, 1919.

material derived from the coal will invav riably condense within the tube itself near the open end. It has beentl'ie practice to determine the amount of the tar thus collected by cutting ofi' the end of the tube in which the tar collects, weighing it, and then washing or burning off the tar and reweighing the tube. The rest of the tube usually has to be broken for the purpose of taking out the coke produced. ,In any event, it is rendered useless for a second distillation.

This makes it impracticable'to use tubes made of expensive material.

The object of the present invention is to provide a distillation tube which may be used repeatedly for many determinations.

\Vith this object in view. the tube is made in two parts, an outer tube, andan inner tube fitting in the outer tube at the'cend in which the tar collects. The inner tube is removable so that itmay be taken out and cleaned of the collected tar. may be used repeatedly, it may be made of expensive refractory material, such as fused silica. quartz, porcelain. etc.

Referring to the embodiment of the invention illustrated in the drawings, the distillation tube 1 comprises an out-er tube 2 and an inner tube 3. The end i of the outer closely in the enlarged part of the outer tube.

and its inner bore forms a-continuation of the inner bore of the part 5 of the outer tube 2.

A stopper 10 of rubber or other material is placed at the end of the outer tube insuch a way as to render the connection between the inner and outer tubes gas-tight. A tar filter 11 fitted onto the stopper in such a way that'one end of the inner tube 3 projects a little way into the filter. The filter is preferably: filled with loose cotton or similar material.

To carry out an experimental coaldistillation. the coal to be tested is placed in the end 5 of the tube. The tubes are connected as shown in Fig. 3, and the open end 12 of the tar filter is connected to a series of ab sorbing apparatus to remove the various volatile by-product-s. Heat is applied to" the Since the tube wall of the enlarged portion 6 of the outer tube 2, but the condensed tarry matter will accumulate inside of the tube 3. If desired,

a portion of the tube 3 maybe packed with a suitable filtering material such as asbestos.

After the distillation is completed the tubes are disconnected, taken-apart and the various by-products determined as usual. To determine the amount of tar collected in the tube 3, the tube 3 is removed and weighed, after which it is washed or burned out and re-weighed.- It may then be replaced in the outer tube for another distillation. The coke remaining in the part 5 may be simply shaken out, because such.

tubes, if made of highly refractory material are not distorted during the process of heating. While it is desirable to have the tube made of a highly refractory material with a low coeiiicient of expansion, the illvention is not restricted to such materlals. 'hile the preferred embodiment of the 111- vention has been specifically illustrated and described, it is to be understood that the invention is not limited to its illustrated embodiment, but may beembodied in other constructions of distillation tubes within the scope of the following claims.

I claim: l. A distillation apparatus, comprising an outer tube in which the material to be distilled is placed, and a removable inner tube seated in the outer tube and forming a lining for the portion of the outer tube in which it seat-s, said inner tube forming a receptacle for the collection of at least a portion of the distillates, substantially as described.

2. A distillation apparatus, comprising an outer tube in which the material to be distilled is placed, and a removable inner tube seated in the outer tube in a manner to prevent leakage around the inner tube and 'to .be distilled and having an enlarged portion, and an inner tube removably seated in said enlarged portion and forming a. lining therefor, said inner tube. forming'a receptacle for the collection of atleast a portion of the distillates, substantially as described.

4.- A distillation apparatus, comprising an outer tube in which the material to be distilled is placed, an inner tube reniovably seated in one end portion of the outer tube, a sealing stopper seated on the adjacent ends of both tubes, and a filter device secured by said stopper and into which the inner tube is arranged to discharge, substantially as described.

5. A tube for experimental coal distillation, comprising an outer tube of refractory silicious material adapted to receive the sample of coal to be distilled. and a removable inner tube fitting closely within one end of the outer tube for the collection of tarry distillates. substantially as described.

6. A tube for experimental coal distillation. comprising an outer tube for receiving the sample of coal to be distilled, a removable inner tube forming a lining for one end portion of the outer tube and projecting therefrom, and a tar filter at the ends of the tubes. the'end of the inner tube projecting into the tar filter, substantially as described.

7. A distillation tube, coi'nprising an outer tube adapted to receive the material to be distilled and having an enlarged portion and a removable inner tube received in said enlarged portion for the collection of a part at least of the distillates, and having sub stantially the same bore as the outer tube; substantially as described.

In testimony whereof, I-have hereunto set my hand. i

lVitnesses H. M. CORWIN,

I GEORGE Panirnnnn. 

